CN105732975A - Method for continuously preparing polyether amine - Google Patents
Method for continuously preparing polyether amine Download PDFInfo
- Publication number
- CN105732975A CN105732975A CN201610249468.3A CN201610249468A CN105732975A CN 105732975 A CN105732975 A CN 105732975A CN 201610249468 A CN201610249468 A CN 201610249468A CN 105732975 A CN105732975 A CN 105732975A
- Authority
- CN
- China
- Prior art keywords
- fluidized
- ammonia
- bed reactor
- hydrogen
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/34—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from hydroxy compounds or their metallic derivatives
- C08G65/48—Polymers modified by chemical after-treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2650/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G2650/28—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type
- C08G2650/50—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule characterised by the polymer type containing nitrogen, e.g. polyetheramines or Jeffamines(r)
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The invention discloses a method for continuously preparing polyether amine and relates to the technical field of hydrogenation and ammoniation of polyether polyol.A fluidized bed reactor is adopted for enabling a catalyst to be in a dynamic state, and contact area between the catalyst and a material; the reaction temperature is stable; the pressure and temperature needed by the reaction are low, side reactions are produced, equipment is easy, and the reaction speed is high; high ammoniation rate and primary amine selectivity are high, the reaction conversion rate is larger than or equal to 99.0%, and the primary amine selectivity is larger than or equal to 99.0%.The catalyst is easier to replace, and has diversified varieties.Excess ammonia gas and nitrogen in the reaction process are recycled, and no pollution is caused to external environment.
Description
Technical field
The present invention relates to the hydrogenation ammonia (amine) of polyether polyol and change technical field, particularly to the method for fluid bed continuously preparing poly ether amines.
Background technology
Polyetheramine (PEA): be a class main chain be polyether structure, end active functional group is the polymer of amido.Polyetheramine is to be reaction raw materials by polyether polyol, and ammonification obtains at high temperature under high pressure.By selecting different polyoxyalkyl structures, a series of performances such as the reactivity of scalable polyetheramine, toughness, viscosity and hydrophilic, and amido is supplied to the probability that polyetheramine reacts with multiple compounds.
Polyether polyol containing terminal hydroxy group is carried out faces hydrogen ammonia (amine) and changes reaction, can preparing a series of aminated compounds, this compounds can be widely used for the fields such as epoxy curing agent, wind power blade firming agent, polyurethane polyureas urea elastomers, gasoline abluent, water base coating, textile finish and epoxy toughening.
Patent CN104693434A discloses the production method of a kind of fixing bed continuity method synthesizing polyether amine, adopts fixed bed reactors to realize continuous prodution polyetheramine；Patent CN104117333A discloses the process units of a kind of continuity method polyetheramine, and employing is that the mode of multiple reactors in series is to realize continuous prodution polyetheramine；Patent CN103524725A discloses the devices and methods therefor of a kind of fixing bed continuous synthesis amine terminated polyether, its technique adopting successive reaction, 1～3 fixing bed, 150 DEG C～300 DEG C, 1～20MPa, ammonia-alcohol ratio 1～15 when reaction, recycle excess of ammonia and hydrogen.Patent CN104119239A discloses a kind of continuity method and produces the technique of small-molecular-weight polyetheramine, adopts the form of the fixing bed of continuity method, adopts the form of 2～6 reactors in series, and improve the conversion ratio of reaction in each reactor equipped with different catalyst.The preparation method that patent CN101522607 discloses a kind of polyetheramine, containing under the metallic framework Raney nickel effects such as cobalt, aluminum, copper, carries out continuous reaction in fixed-bed tube reactor.
Patent CN102408559A discloses the preparation technology of a kind of amine terminated polyether, the method with number-average molecular weight be more than 100 polyether polyol for raw material, under hydrogen, aminating agent and skeletal nickel catalyst exist, in autoclave, prepare polyetheramine by catalysis reduction amination；Patent CN102336903A discloses the production method of a kind of aliphatic poly ether amines and the preparation of special-purpose catalyst thereof, its catalyst is frame special Raney nickel, and the method adopts in autoclave is faced hydrogen ammonification synthesizing polyether amine by polyether polyol under frame special Raney nickel.
What method made above adopted is batch process production or the serialization fixed-bed approach of reaction under high pressure autoclave.And batch tank method product all exists quality instability, side reaction is many, not easily realizes the shortcomings such as Automated condtrol；Serialization fixed-bed approach by contrast relatively batch tank method constant product quality, side reaction, it easily is automated control, but above-mentioned continuity method adopts fixed bed type reactor, there is equipment complexity, catalyst change is difficult, produce the shortcoming that kind is single.
Summary of the invention
Goal of the invention is in that to provide a kind of energy amination rate height, primary amine selectivity is good, technique is simple, catalyst is easily changed, the method for the fluid bed continuously preparing poly ether amines of the changeable production multi items of same set of device.
The technical scheme is that: the upper top at fluidized-bed reactor arranges nebulizer, at the middle part of fluidized-bed reactor, skeletal nickel catalyst is set, in fluidized-bed reactor, ammonia, hydrogen mixed gas distributor are set in skeletal nickel catalyst bottom, liquid distribution trough is set in fluidized-bed reactor bottom；Polyether polyol through preheating is sprayed on skeletal nickel catalyst continuously through nebulizer, in temperature is 130 DEG C～250 DEG C and pressure is 3～6MPa when, faces hydrogen aminating reaction；Fluidized-bed reactor upper end outlet passes through gas-liquid separator separates water outlet, and isolated ammonia, hydrogen mixed gas are entered fluidized-bed reactor by ammonia, hydrogen mixed gas distributor after compressor and fresh ammonia, hydrogen adjust mixing ratio；Liquid distribution trough collects the reactant mixture of fluidized-bed reactor, and through the upper end of circulating pump reflux again to skeletal nickel catalyst, the polyetheramine of acquirement is collected in product collecting tank through circulating pump.
Compared with prior art, the present invention adopts fluid bed reactor catalysis agent to be in dynamically, adds contacting of catalyst and material；Reaction temperature is steady；Pressure and the temperature of reaction needed are low, and side reaction is few, and equipment is simple, and response speed is fast；There is higher ammonification rate, high primary amine selectivity, reaction conversion ratio >=99.0%, primary amine selectivity >=99.0%；Catalyst is more easy to replacing, diversification of varieties；Excessive gaseous ammonia and hydrogen in course of reaction recycle, and environment realizes no pollution to external world.
Further, the molecular weight of polyether polyol of the present invention is 200～5000, the main chain of polyether polyol is containing at least any one copolymer in polypropylene glycol, Polyethylene Glycol, containing 1～3 hydroxyl in polyether polyol, it is possible to produce multi-series kind by this device.
Additionally, the mixing mol ratio of described polyether polyol and ammonia is 1: 30～100, the present invention adopts higher ammonia alcohol mol ratio to be conducive to aminating reaction to carry out to positive reaction direction, enable polyether polyol fully, continuous print carry out aminating reaction, course of reaction is evenly distributed, side reaction is few, improves ammonification rate.
From described ammonia, the distribution of hydrogen mixed gas distributor ammonia, in hydrogen mixed gas, hydrogen volume accounting is 4～20%, and the present invention adopts higher hydrogen ratio to be conducive to polyether polyol can complete the reaction of dehydrogenation after first hydrogenation fully, improves the selectivity of primary amine；And the color and luster of product can be reduced.
Ammonia, hydrogen mixed gas circular flow be 500～2000m3/h.The present invention adopts bigger circular flow, it is possible to strengthen hydrogen, ammonia contacts with polyether polyol, thus improving ammonification rate and selectivity.
In described fluidized-bed reactor, skeletal nickel catalyst loading accounts for the 20～50% of fluidized-bed reactor volume.The present invention adopts this more catalyst to exist in system, it is possible to improve the activity of reaction, accelerates response speed, shortens the polyether polyol time in fluidized-bed reactor, improves the yield of each hour.
Accompanying drawing explanation
Fig. 1 is the production technology schematic diagram of the present invention.
Detailed description of the invention
One, preparation is set:
As it is shown in figure 1, the upper top at fluidized-bed reactor 1 arranges nebulizer 7, at the middle part of fluidized-bed reactor 1, skeletal nickel catalyst 1-1 is set by catalyst inlet and outlet.In fluidized-bed reactor 1, ammonia, hydrogen mixed gas distributor 9 are set in skeletal nickel catalyst 1-1 bottom, also set up liquid distribution trough 8 in fluidized-bed reactor 1 bottom.
Gas-liquid separator 2 is connected above through pipeline at fluidized-bed reactor 1, gas-liquid separator 2 be provided above ammonia, hydrogen mixed export, this ammonia, hydrogen mixed export are connected to the entrance of a recycle compressor 3 again through pipeline, on this pipeline, also the other fresh hydrogen that connects fills into mouth and fresh ammonia fills into mouth, and the outlet of recycle compressor 3 is connected to the entrance point of ammonia, hydrogen mixed gas distributor 9.Gas-liquid separator 2 is arranged below Water Sproading mouth, and is connected with water collecting tank 5 by pipeline.
Circulating pump 4 is set outside fluidized-bed reactor 1, the import of circulating pump 4 is connected to the port of export of liquid distribution trough 8, the outlet of circulating pump 4 connects two switch valves respectively by threeway, the other end of one switch valve is by above the skeletal nickel catalyst 1-1 in pipeline incoming stream fluidized bed reactor 1, and the other end of another switch valve is practiced midwifery product collecting tank 6 by pipeline.
Two, example is produced:
Embodiment 1:
Polypropylene glycol ether (molecular weight is 230) is continuously entered the fluidized-bed reactor 1 that be loaded with skeletal nickel catalyst 1-1 (catalyst loading account for fluidized-bed reactor volume 50%) through the nebulizer 7 at fluidized-bed reactor 1 top from top after preheater is warming up to 130 DEG C in advance, and hydrogen (hydrogen source through Pressure-stabilizing pressure reducing device decompressing and continuous provide, keep hydrogen concentration in systems be 20%) and ammonia (the mixing mol ratio of polypropylene glycol ether and ammonia is 1: 100) pass into fluidized-bed reactor by recycle compressor 3 from bottom, hydrogen aminating reaction is faced in temperature is 130 DEG C and pressure is 6MPa when.Reactor top reactant separates water outlet and ammonia, hydrogen through gas-liquid separator 2, and the ammonia of separation, hydrogen mixed gas regulate mixing through compressor 3 and fresh hydrogen, ammonia gaseous mixture, and be again introduced in fluidized-bed reactor 1 keeping ammonia hydrogen circulating air flow is 2000m3/h；Bottom fluidized-bed reactor 1, a reactant part is recycled to fluidized-bed reactor 1 continuation reaction, a part of continuous discharge, obtains bifunctional molecule and measure the polyetheramine product of 230 in product collecting tank 6.
Reaction conversion ratio 99.32% after testing, primary amine selectivity >=99.15%.
Embodiment 2:
Polypropylene glycol ether (molecular weight is 2000) is continuously entered the fluidized-bed reactor that be loaded with skeletal nickel catalyst (catalyst loading account for fluidized-bed reactor volume 20%) through the nebulizer at fluidized-bed reactor top from top after preheater is warming up to 170 DEG C in advance, and hydrogen (hydrogen source through Pressure-stabilizing pressure reducing device decompressing and continuous provide, keep hydrogen concentration in systems be 4%) and ammonia (the mixing mol ratio of polypropylene glycol ether and ammonia is 1: 30) pass into fluidized-bed reactor by recycle compressor from bottom, hydrogen aminating reaction is faced in temperature is 170 DEG C and pressure is 3MPa when.Reactor top reactant is through gas-liquid separator separates water and ammonia, hydrogen, and the ammonia of separation, hydrogen mixed gas mix through compressor and fresh gaseous mixture, and be again introduced in reactor keeping ammonia hydrogen circulating air flow is 500m3/h；A reactor bottom reactant part is recycled to fluidized-bed reactor and continues reaction, and a part of continuous discharge obtains bifunctional molecule and measures the polyetheramine product of 2000.
Reaction conversion ratio 99.63% after testing, primary amine selectivity >=99.58%.
Embodiment 3:
Trimethylolpropane polypropylene glycol ether (molecular weight is 430) is continuously entered the fluidized-bed reactor that be loaded with skeletal nickel catalyst (catalyst loading account for fluidized-bed reactor volume 40%) through the nebulizer at fluidized-bed reactor top from top after preheater is warming up to 200 DEG C in advance, and hydrogen (hydrogen source through Pressure-stabilizing pressure reducing device decompressing and continuous provide, keep hydrogen concentration in systems be 15%) and ammonia (the mixing mol ratio of trimethylolpropane polypropylene glycol ether and ammonia is 1: 80) pass into fluidized-bed reactor by recycle compressor from bottom, hydrogen aminating reaction is faced in temperature is 200 DEG C and pressure is 5MPa when.Reactor top reactant is through gas-liquid separator separates water and ammonia, hydrogen, and the ammonia of separation, hydrogen mixed gas mix through compressor and fresh gaseous mixture, and be again introduced in reactor keeping ammonia hydrogen circulating air flow is 1800m3/h；A reactor bottom reactant part is recycled to fluidized-bed reactor and continues reaction, and a part of continuous discharge obtains the polyetheramine product of trifunctional molecule amount 430.
Reaction conversion ratio 99.28% after testing, primary amine selectivity >=99.06%.
Embodiment 4:
Nonyl phenol polypropylene glycol ether (molecular weight is 1000) is continuously entered the fluidized-bed reactor that be loaded with skeletal nickel catalyst (catalyst loading account for fluidized-bed reactor volume 25%) through the nebulizer at fluidized-bed reactor top from top after preheater is warming up to 180 DEG C in advance, and hydrogen (hydrogen source through Pressure-stabilizing pressure reducing device decompressing and continuous provide, keep hydrogen concentration in systems be 8% and ammonia (the mixing mol ratio of nonyl phenol polypropylene glycol ether and ammonia is by recycle compressor from bottom pass into fluidized-bed reactor at 1: 40, hydrogen aminating reaction is faced in temperature be 180 DEG C of pressure is 4MPa when.Reactor top reactant is through gas-liquid separator separates water and ammonia, hydrogen, the ammonia, the hydrogen mixed gas that separate mix through compressor and fresh gaseous mixture, be again introduced in reactor keeping ammonia hydrogen circulating air flow is 600m3/h, a reactor bottom reactant part is recycled to fluidized-bed reactor and continues reaction, and a part of continuous discharge obtains mono-functional molecule and measures the polyetheramine product of 1000.
Reaction conversion ratio 99.71% after testing, primary amine selectivity >=99.37%.
Embodiment 5:
Glycerol polypropylene glycol ether (molecular weight 5000) is continuously entered the fluidized-bed reactor that be loaded with skeletal nickel catalyst (catalyst loading account for fluidized-bed reactor volume 30%) through the nebulizer at fluidized-bed reactor top from top after preheater is warming up to 250 DEG C in advance, and hydrogen (hydrogen source through Pressure-stabilizing pressure reducing device decompressing and continuous provide, keep hydrogen concentration in systems be 10%) and ammonia (the mixing mol ratio of glycerol polypropylene glycol ether and ammonia is 1: 50) pass into fluidized-bed reactor by recycle compressor from bottom, hydrogen aminating reaction is faced in temperature is 250 DEG C and pressure is 6MPa when.Reactor top reactant is through gas-liquid separator separates water and ammonia, hydrogen, and the ammonia of separation, hydrogen mixed gas mix through compressor and fresh gaseous mixture, and be again introduced in reactor keeping ammonia hydrogen circulating air flow is 1000m3/h；A reactor bottom reactant part is recycled to fluidized-bed reactor and continues reaction, and a part of continuous discharge obtains the polyetheramine product of trifunctional molecule amount 5000.
Reaction conversion ratio 99.53% after testing, primary amine selectivity >=99.27%.
Embodiment 6:
Polyethylene Glycol polyethylene glycol block polyethers (molecular weight is 600) is continuously entered the fluidized-bed reactor that be loaded with skeletal nickel catalyst (catalyst loading account for fluidized-bed reactor volume 35%) through the nebulizer at fluidized-bed reactor top from top after preheater is warming up to 220 DEG C in advance, and hydrogen (hydrogen source through Pressure-stabilizing pressure reducing device decompressing and continuous provide, keep hydrogen concentration in systems be 18% and ammonia (the mixing mol ratio of Polyethylene Glycol polyethylene glycol block polyethers and ammonia is that 1:90 passes into fluidized-bed reactor by recycle compressor from bottom, hydrogen aminating reaction is faced in temperature be 220 DEG C of pressure is 5MPa when.Reactor top reactant is through gas-liquid separator separates water and ammonia, hydrogen, the ammonia, the hydrogen mixed gas that separate mix through compressor and fresh gaseous mixture, be again introduced in reactor keeping ammonia hydrogen circulating air flow is 1300m3/h, a reactor bottom reactant part is recycled to fluidized-bed reactor and continues reaction, and a part of continuous discharge obtains bifunctional molecule and measures the polyetheramine product of 600.
Reaction conversion ratio 99.18% after testing, primary amine selectivity >=99.15%.
Embodiment 7:
Methoxy poly (ethylene glycol) polypropylene glycol ether (molecular weight is 2000) is continuously entered the fluidized-bed reactor that be loaded with skeletal nickel catalyst (catalyst loading account for fluidized-bed reactor volume 25%) through the nebulizer at fluidized-bed reactor top from top after preheater is warming up to 150 DEG C in advance, and hydrogen (hydrogen source through Pressure-stabilizing pressure reducing device decompressing and continuous provide, keep hydrogen concentration in systems be 6% and ammonia (the mixing mol ratio of methoxy poly (ethylene glycol) polypropylene glycol ether and ammonia is by recycle compressor from bottom pass into fluidized-bed reactor at 1: 35, hydrogen aminating reaction is faced in temperature be 150 DEG C of pressure is 4.5MPa when.Reactor top reactant is through gas-liquid separator separates water and ammonia, hydrogen, the ammonia, the hydrogen mixed gas that separate mix through compressor and fresh gaseous mixture, be again introduced in reactor keeping ammonia hydrogen circulating air flow is 800m3/h, a reactor bottom reactant part is recycled to fluidized-bed reactor and continues reaction, and a part of continuous discharge obtains mono-functional molecule and measures the polyetheramine product of 2000.
Reaction conversion ratio 99.67% after testing, primary amine selectivity >=99.54%.
Embodiment 8:
Polyethylene Glycol polyethylene glycol block polyethers (molecular weight is 900) is continuously entered the fluidized-bed reactor that be loaded with skeletal nickel catalyst (catalyst loading account for fluidized-bed reactor volume 40%) through the nebulizer at fluidized-bed reactor top from top after preheater is warming up to 160 DEG C in advance, and hydrogen (hydrogen source through Pressure-stabilizing pressure reducing device decompressing and continuous provide, keep hydrogen concentration in systems be 12% and ammonia (the mixing mol ratio of Polyethylene Glycol polyethylene glycol block polyethers and ammonia is by recycle compressor from bottom pass into fluidized-bed reactor at 1: 70, hydrogen aminating reaction is faced in temperature be 160 DEG C of pressure is 5.5MPa when.Reactor top reactant is through gas-liquid separator separates water and ammonia, hydrogen, the ammonia, the hydrogen mixed gas that separate mix through compressor and fresh gaseous mixture, be again introduced in reactor keeping ammonia hydrogen circulating air flow is 1600m3/h, a reactor bottom reactant part is recycled to fluidized-bed reactor and continues reaction, and a part of continuous discharge obtains bifunctional molecule and measures the polyetheramine product of 900.
Reaction conversion ratio 99.37% after testing, primary amine selectivity >=99.25%.
Claims (6)
1. the method for a continuously preparing poly ether amines, it is characterized in that: the upper top at fluidized-bed reactor arranges nebulizer, at the middle part of fluidized-bed reactor, skeletal nickel catalyst is set, in fluidized-bed reactor, ammonia, hydrogen mixed gas distributor are set in skeletal nickel catalyst bottom, liquid distribution trough is set in fluidized-bed reactor bottom；Polyether polyol through preheating is sprayed on skeletal nickel catalyst continuously through nebulizer, in temperature is 130 DEG C～250 DEG C and pressure is 3～6MPa when, faces hydrogen aminating reaction；Fluidized-bed reactor upper end outlet passes through gas-liquid separator separates water outlet, and isolated ammonia, hydrogen mixed gas are entered fluidized-bed reactor by ammonia, hydrogen mixed gas distributor after compressor and fresh ammonia, hydrogen adjust mixing ratio；Liquid distribution trough collects the reactant mixture of fluidized-bed reactor, and through the upper end of circulating pump reflux again to skeletal nickel catalyst, the polyetheramine of acquirement is collected in product collecting tank through circulating pump.
2. preparation method according to claim 1, it is characterised in that the molecular weight of described polyether polyol is 200～5000, the main chain of polyether polyol is containing at least any one copolymer in polypropylene glycol, Polyethylene Glycol, containing 1～3 hydroxyl in polyether polyol.
3. preparation method according to claim 1, it is characterised in that the mixing mol ratio of described polyether polyol and ammonia is 1: 30～100.
4. preparation method according to claim 1, it is characterised in that in described ammonia, the ammonia of hydrogen mixed gas distributor distribution, hydrogen mixed gas, hydrogen volume accounting is 4～20%.
5. preparation method according to claim 1, it is characterised in that ammonia, hydrogen mixed gas circular flow be 500～2000m3/h。
6. preparation method according to claim 1, it is characterised in that in described fluidized-bed reactor, skeletal nickel catalyst loading accounts for the 20～50% of fluidized-bed reactor volume.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610249468.3A CN105732975B (en) | 2016-04-21 | 2016-04-21 | A kind of method of continuously preparing poly ether amines |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610249468.3A CN105732975B (en) | 2016-04-21 | 2016-04-21 | A kind of method of continuously preparing poly ether amines |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105732975A true CN105732975A (en) | 2016-07-06 |
| CN105732975B CN105732975B (en) | 2018-01-09 |
Family
ID=56254981
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610249468.3A Active CN105732975B (en) | 2016-04-21 | 2016-04-21 | A kind of method of continuously preparing poly ether amines |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105732975B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106633029A (en) * | 2017-01-04 | 2017-05-10 | 扬州晨化新材料股份有限公司 | Method of continuously preparing polyether amines |
| CN108727580A (en) * | 2017-04-21 | 2018-11-02 | 中国石油化工股份有限公司 | A kind of vulcanization bed reaction technique preparing amine terminated polyether |
| CN113603880A (en) * | 2021-09-10 | 2021-11-05 | 扬州晨化新材料股份有限公司 | System and method for continuously producing low molecular weight polyether amine |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104231256A (en) * | 2014-10-13 | 2014-12-24 | 南京红宝丽股份有限公司 | Continuous preparation method of amine-terminated polyether |
-
2016
- 2016-04-21 CN CN201610249468.3A patent/CN105732975B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104231256A (en) * | 2014-10-13 | 2014-12-24 | 南京红宝丽股份有限公司 | Continuous preparation method of amine-terminated polyether |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106633029A (en) * | 2017-01-04 | 2017-05-10 | 扬州晨化新材料股份有限公司 | Method of continuously preparing polyether amines |
| CN106633029B (en) * | 2017-01-04 | 2018-08-17 | 扬州晨化新材料股份有限公司 | A kind of method of continuously preparing poly ether amines |
| CN108727580A (en) * | 2017-04-21 | 2018-11-02 | 中国石油化工股份有限公司 | A kind of vulcanization bed reaction technique preparing amine terminated polyether |
| CN108727580B (en) * | 2017-04-21 | 2021-04-06 | 中国石油化工股份有限公司 | Fluidized bed reaction process for preparing amino-terminated polyether |
| CN113603880A (en) * | 2021-09-10 | 2021-11-05 | 扬州晨化新材料股份有限公司 | System and method for continuously producing low molecular weight polyether amine |
| CN113603880B (en) * | 2021-09-10 | 2022-08-05 | 扬州晨化新材料股份有限公司 | System and method for continuously producing low molecular weight polyether amine |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105732975B (en) | 2018-01-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104693434A (en) | Production method for continuously synthesizing polyether amine through static bed | |
| CN105732975B (en) | A kind of method of continuously preparing poly ether amines | |
| CN103524725B (en) | The devices and methods therefor of fixed bed continuous synthesis Amino Terminated polyether(ATPE) | |
| CN104231256B (en) | A kind of continuous preparation method of amine terminated polyether | |
| CN107880260B (en) | Continuous preparation device and preparation method of small molecular weight amino-terminated polyether | |
| CN113603880B (en) | System and method for continuously producing low molecular weight polyether amine | |
| CN109715610A (en) | The method that polyamine is prepared by dintrile and/or amino nitrile | |
| CN104419002B (en) | A kind of production method of amine terminated polyether | |
| CN110327931B (en) | Catalyst, preparation method thereof and production process of propyleneamine using catalyst | |
| CN102503909A (en) | Compound containing tertiary amine derivatives, preparation method and application thereof | |
| CN104475118A (en) | Supported Ni-Cu-Cr catalyst and application thereof | |
| CN205556526U (en) | Device of serialization preparation polyetheramine | |
| CN106633029B (en) | A kind of method of continuously preparing poly ether amines | |
| CN113149850A (en) | Process for continuously preparing N-hydroxyethyl-1, 3-propane diamine by using micro-mixing and fixed bed reactor | |
| CN114276533A (en) | Method and device for continuously preparing polyether amine | |
| CN109569441A (en) | A kind of method of reactor and serialization preparation small molecule polyetheramine | |
| CN115449068B (en) | Method for preparing amino-terminated polyether by continuous hydro-ammonification | |
| CN115178191A (en) | Polyether amine continuous production system and method | |
| CN101544570B (en) | Method for preparing m-phenylene dimethylamine | |
| CN108727580B (en) | Fluidized bed reaction process for preparing amino-terminated polyether | |
| CN106040253A (en) | Preparation method and application of primaquine-terminated polyether catalyst prepared through static bed catalytic hydrogenation | |
| CN112961061B (en) | Process for preparing N-methyl-1, 3-propane diamine by continuous catalytic reaction of two fixed bed reactors | |
| CN206435169U (en) | A kind of integral reactor for preparing polyetheramine | |
| CN211586542U (en) | Continuous hydroamination reaction device | |
| CN105713191A (en) | Technology for producing polyether amine through continuous hydrogen ammonification |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |